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Agricultural Sciences in China

2007, 6(12): 1487-1493

ScienceDirect

December 2007

Study on Aroma Components in Fruit From Three Different Satsuma Mandarin

Varieties
QIAO Yu, XIE Bi-jun, ZHANG Yan, ZHOU Hai-yan and PAN Si-yi
College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, P.R.China

Abstract
Fruit aroma of Guoqing 1, Miyagawa Wase, and Owari from three different Satsuma mandarin varieties were investigated
by headspace solid phase microextraction (HS-SPME) combined with GC-MS. The results showed that there were 73, 71,
and 66 aroma components in the three varieties, and the total contents were 584.67, 505.29, and 494.63 yg g-1, respectively.
Total 29 constituents were common in the three varieties. It was also found that Guoqing 1, Miyagawa Wase, and Owari
had 12, 5, and 2 unique components, respectively. The key aroma components were limonene, linalool, y-terpinene, pmyrcene, a-pinene, and octanal in the three fruits. Guoqing 1 contained more key aroma compounds than Miyagawa
Wase and Owari.

Key words: Satsuma mandarins, fruit, volatile compounds, aroma

INTRODUCTION
Aroma is one of the most important quality attributes
of citrus fruit and the most significant parameter of
quality in both eatable and processed products. In order to improve the fruit quality and modify the aroma
formation, information on the flavor constitution present
in fruit is needed and important for cultivar breeding
and further processing. Researches on citrus aroma
have been performed for many years in western
countries. Aroma of grapefruit juice and sweet orange
juice which were the major processing cultivars has
been extensively investigated and reviewed (N6nez
et al. 1985; Nisperos-Carried0 and Shaw 1990; Shaw
and Moshonas 1997; Jia et al. 1998; Tgnder et al. 1998;
Bazemore et al. 1999; Jordan et al. 2001, 2003; Lin
et al. 2002; Rega et al. 2003; Moufida and Marzouk
2003; Selli et al. 2004; Allegrone et al. 2006; Arena

et al. 2006). Many studies on aroma of juice and essential oil have been conducted on Satsuma mandarins
(Yajima et al. 1979; Ohta et al. 1982; Moshonas and
Shaw 1997; Minh et al. 2002; PCrez et al. 2005; PCrezL6pez and Carbonell-Barrachina 2006), but few data
exist on the fruit aroma. Elmaci and Altug (2005) detected 26 volatile compounds in the three mandarin cultivars from Turkey using dynamic headspace and found
the key aroma impact compounds were limonene, yterpinene, p-cymene, myrcene, a-pinene, P-pinene, and
a-terpinolene in all samples by sensory evaluation.
In China, Satsuma mandarins, originating in
Huangyan and Wenzhou of Zhejiang Province, are distributed widely and have the highest yield. Mandarins
are primarily consumed as fresh fruit and processed
into tin cans in industry. Although Satsuma mandarins
possess the important economic values with respect to
the citrus industry in China, only volatile compounds
of essential oil from Satsuma mandarins were previ-

This paper is translated from its Chinese version in Scientia Agricultura Sinica.
QIAO Yu.Ph D candidate, E-mail: qiaoyu412@sina.com;Correspondence PAN Si-yi, Professor, Tel: +86-27-87283778, E-mail: pansiyiOmail.hzau.edu.cn

02007, CAAS. All rights resewed. Publishedby Elsevler Ltd.

QIAO Yu et al.

1488

ously reported (Huang and Wu 1998; Shan and Li 2006;

Zhang et al. 2007; Zhou et al. 2007). Relatively little
information is available on the flavor of Chinese Satsuma mandarins (Zhou et al. 2007), especially the native cultivar grown in China.
In the present study, aroma of Guoqing 1, Miyagawa
Wase, and Owari, the three different Satsuma mandarin varieties from the Songzi region of China, were investigated by headspace solid phase microextraction
(HS-SPME) combined with GC-MS. By determining
the volatile components from the three fruits, we can
have a better perspective on the characteristic aroma
compounds in different cultivars and get some information on cultivar breeding and juice processing.

MATERIALS AND METHODS

Materials
The samples of Guoqing 1 (Citrus unshiu Marc. cv.
Guoqing 1). Miyagawa Wase (Citrus unshiu Marc. cv.
Miyagawa Wase), and Owari (Citrus unshiu Marc. cv.
Owari) fruits from citrus garden, located in the Songzi
region of Hubei Province, China, were collected on October 11, October 31, and November 9 in 2006,
respectively. The total soluble solids of Guoqing 1,
Miyagawa Wase, and Owari were 9, 11, and 12.5%
and total soluble solids/total acidity ratioes (TSS/TA)
were 13.24, 14.67, and 12.25, respectively. Analysis
of volatile compounds was carried out after 24 h in the
wake of postharvest.

tracted by DVB/CAR/PDMS fiber for 40 min at the

same temperature under stirring. After extraction, the
fiber was inserted into the injection port of GC to desorb the analytes for 5 min.
GC-MS analysis GC-MS was carried out using a HP
5975C quadropole mass selective detector at 150C
(Agilent Technologies, USA). Mass spectral ionization
was set at 230C. The mass spectrometer was operated in the electron ionization mode at a voltage of 70
eV. The flow rate of helium on HP-5 column (30 m x
0.25 mm i.dx 0.25 pm film thickness, J&W Scientific,
Folsom, CA, USA) is 1 mL min-'. Analysis was performed in the splitless mode and injector temperature
was 250C. The column was held at 35C for 5 min,
then increased from 35 to 180C at 3C min-I, held at
180C for 1 min, and finally increased to 240C at a
rate of 5C m i d , held for 5 min.
Volatile components were tentatively identified by
comparing their mass spectra with the mass spectra of
libraries (NISTOS, WILEY7.0) and references
(Moshonas and Shaw 1997; Jordan et al. 2001,2003;
Lin et al. 2002). Semiquantificationof compounds identified in this study was calculated by comparing the
peak area of each compound with that of the internal
standard.

RESULTS
Total ionic chromatograms of volatile compounds in
the three different Satsuma mandarin fruits are shown
in Fig. and Table 1, indicating the quality and quantity
results of components.

Methods
Determination of the volatile compounds of Satsuma mandarins 4 kg fruit of each cultivar were
peeled and reamed in a centrifugejuice extraction. The
3 g pulp with 3.6 g NaC1, previously added to 1 p L of
IS solution (cyclohexanoe), was placed into a 20-mL
vial containing a microstirring bar. The SPME manual
device equipped with a 50/30 pm DVB/CAR/PDMS fiber (Supelco, Bellfonte, PA, USA) was used for extraction of orange juice. The fiber was conditioned in
GC injector port at 270C for 1 h prior to use. The
sample was equilibrated at 40C for 15 min and ex-

The aroma compounds of the three different

Satsuma mandarins
The identified volatile compounds and their relative
amounts are given in Tables 1 and 2. Differences in the
composition of volatile molecules from Guoqing 1,
Miyagawa Wase, and Owari were observed.
A total of 65 components were identified in Guoqing 1
fruit and their total concentration was 584.67 pg g-'. The
highest amounts of volatile compounds were limonene,
linalool, y-terpinene, P-myrcene, octanal, decanal,
terpinen-4-01, and (E)-Zhexen-l-ol.

02007,CAAS.All dghts reserved.Publishedby Elsevier Ltd.

Study on Aroma Components in Fruit From Three Different Satsuma Mandarin Varieties

1489

Table 1 Volatile compounds from three different Satsuma mandarin varieties

Compounds
Hydrocarbons
a-Thujene
a-Pinene
Camphene
Sahinene
P-Pinene
P-Myrcene
3-Carene
a-Terpinene
D-Limonene
(Z)-b-Ocimene
y-Terpinene
Terpinolene
l-Methyl-4-(1-methylethenyl)-henzne
GElemene
a-Cuhehene
Copaene
P-Cubebene
P-Elemene
Junipene
P-Caryophyllene
p-Gurjunene
a-Caryophyllene
Isoledene
y-Muurolene
Cermacrene D
P-Humulene
Valencene
a-Selinene
a-Amorphene
GAmorphene
A 1coho 1s
Ethyl alcohol
(Z)-Z-Hexen-1-01
(E)-Z-Hexen-1-01
I-Octanol
Linalool
trans-p-Mentha-2.8-diene-1-01
Isopulegol
P-Terpinol
Borneo1

Content (pg g-1)

Guoaine 1 Mivaeawa Wase
0.17
0.90
0.02
0.50
0.84
8.95

0.34
1 .oo

0.59
1.29
8.41
0.46

Owari
0.14
0.79
0.02
0.36
0.74
7.76

0.55

462.89
I .93
21.12
1.28
0.3 I

0.07
0.16
0.26
0.09
0.39
0.03
0.23
0.04
0.12
0.04
0.05
0.24
0.06
0.70
0.13
0.05
0.25

422.31
1.71
19.10
1.56
0.23

0.3 I
0.1 1

400.60
1.60
17.30
1.02
0.05
0.04
0.10
0.17
0.06
0.19
0.14
0.06
0.03

1.13

0.20

0.21

0.71

0.17

2.13
1.34
50.54
1.20
0.33

I .42

26.45
0.46
0.28

1.15
0.26
5.39
0.95
36.36
0.44
0.28
0.08

Compounds

Content (pg g-')

Guoqing I
Miyagawa Wase
0.21
2.49
I .84
2.95
1.15
0.40
0.37
0.47
0.27
0.18

I-Nonanol
4-Terpineol
a-Terpineol
cis-Carveol
Nerol
Citronellol
Geraniol
Thymol
Aldehydes
Hexanal
(E)-Z-Hexenal
Heptanal
Octanal
Nonanal
Citronella1
Decanal
Neral
(Z)-2-Decenal
(E)-Z-Decenal
Geranial
Perillal
Undecanal
2-Undecenal
(E,E)-Zd-Decadienal
Esters
Butyl hutanoate
Ethyl hexanoate
Ethyl octanoate
Linalyl acetate
Citronellyl acetate
Neryl acetate
Geranyl acetate
Isopropyl Myristate
Ketones
Camphor
Carvone
(Z)-6,IO-Dimethyl-5,9-undecadien-2-one
@)-6,1O-Dimethyl-5,9-undecadien-2-one
Acids
Acetic acid

1.19
0.43
0.14
8.81
0.21
3.07
0.84

1.02
0.14
7.93
0.98
1.49

Owari
2.06
1.98
0.24
0.25
0.15
0.06
0.68
0.10
0.16
7.05
0.08
I .76
0.48

0.52
0.12
0.64
0.34

0.34
0.23

0.07
0.39
0.25

0.11

0.16
0.54
0.25
0.42
0.1 I
0.29
0.20
0.66
0.32

0.24

0.72

0.42
0.08
0.21
0.12
0.41
0.2 I

0.27
0.17
0.73
0.02
0.13

0.65

0.16
0.59
0.12
0.07

0.05

-.not found or not exist.

There were 36 components found in Miyagawa
Wase fruit and the concentration of the total volatiles
was 505.29 pg g-I. The most abundant compounds
were limonene, Iinalool, y-terpinene, P-myrcene, octanal,
terpinen-4-01, (Z)-p-ocimene, terpinolene, and decanal.
Fifty-five compounds were determined in Owari fruit
and the total concentration was 494.63 pg g-*. The
major volatile compounds were limonene, linalool, yterpinene, P-myrcene, octanal, (E)-2-hexen- 1-01,
terpinen-4-01, and decanal.
Guoqing 1 had the most kinds and greatest amounts
of aroma compounds in all samples. Total 29 common
constituents were found in the three varieties. Guoqing
1 had 12 unique compounds, which were P-gurjunene,
isoledene, germacrene D, P-humulene, a-selinene, aamorphene, borneol, 1-nonanol, nerol, undecanal, bu-

tyl butanoate, and (2)-6,1O-dimethyl-5,9-undecadien2-one. 3-Carene, a-terpinene, nonanal, 2-undecenal,

and (E,E)-2,4-decadienal were found only in Miyagawa
Wase, while (Z)-2-hexen-1-01and P-terpinol were detected only in Owari fruit.

Comparison of volatile constitution in the three

different Satsuma mandarinvarieties
Hydrocarbons Hydrocarbons, especially the monoterpene hydrocarbons, are the highest amount group in
citrus aroma. The most abundant group of volatile compounds in the three selected Satsuma mandarin fruits
were hydrocarbons, and the monoterpene hydrocarbons presented in higher quantities than sesquiterpene
hydrocarbons.

02007,CMS. All rights resewed. Published by ElsevierLtd.

QIAO Yu et (11.

1490

A
3 800000

%
B

'z

-2

3 600 000
3 400 000
3 200 000
3 000 000
2800000
2600000
2400000
2200000
2000000
1800000
1600000

I400000
1200000
1 000 000 i

Time (min)

&
0

50.00

55.00

60.00

Time (min)

Time (min)

Fig. Total ionic chromatograms of volatile compounds in the three different Satsuma mandarins fruits. A, Guoqing 1; B, Miyagawa Wase;
c, owari.

The most abundant compounds in the three mandarin fruits were limonene (462.893, 422.313, and
400.603 pg g-', respectively) followed by y-terpinene
and P-myrcene.
Valencene, which was detected in the highest amounts

in Miyagawa Wase, was the sesquiterpene component

found in greatest concentrations in all samples, representing about 0.04-0.22%of total contents.
Alcohols Alcohols have been described to be the most
important contributors to citrus flavor, especially ter-

02007, CAAS. All rights resewed. Publishedby ElsevierLtd.

Study on Aroma Components in Fruit From Three Different Satsuma Mandarin Varieties

Table 2 Compounds and contents of aroma components in the

three different Satsuma mandarin varieties
Compounds
Hydrocarbons
Monoterpenes
Sesquiterpenes
Others
Alcohols
Aliphatic alcohols
Terpene alcohols
Others
Aldehydes
Aliphatic aldehydes
Terpene aldehydes
Esters
Ketones
Acids
Total

Guoqing 1
501.83
499.06
2.43
0.34
63.64
4.39
58.59
0.66
15.90
13.87
2.03
2.26
1.04
0
584.67

Content (pg g-1)

Miyagawa Wase
459.09
457.62
1.24
0.23
31.77
1.59
30.18
0
13.37
12.8
0.57
0.4 I
0.65
0
505.29

Owari
43 1.59
430.56
0.98
0.05
49.63
7.75
41.58
0.3 I
11.01
9.82
1.19
1.46
0.87
0.07
494.63

pene alcohols have the characteristic aroma. These

compounds were found to account for 0.06% in
Miyagawa Wase, lower than in Guoqing 1 and Owari.
The dominant alcohol was linalool, with the highest
content in Guoqing 1 (50.54 pg g-I). Except for (E)2-hexen- 1-01, alcohol components are found in higher
quantities in Guoqing 1 than other varieties. The key
aroma compounds of citrus such as cis-carveol, nerol,
citronellol, and geraniol were not detected in
Miyagawa Wase.
Aldehydes Aldehydes are also the main aroma compounds in citrus. The aliphatic aldehydes are found
in lower quantities than terpene aldehydes. Octanal
was found in considerable quantities (8.81, 7.93, and
7.05 pg g-I, respectively). Miyagawa Wase contained
the lower quantities of terpene aldehydes, only representing 0.11 %. The quantities of hexanal, decanal,
neral, and geranial in Owari were less than those of
Guoqing 1. Moreover, several unsaturated aldehydes
with long carbonate chains were found, such as
undecanal in Guoqing 1 and 2-undecenal in Miyagawa
Wase.
Esters Esters presenting fruity note in trace amounts
have been considered very important to citrus flavor.
The contents of esters in the three variety fruits were
0.39, 0.08, and 0.30%,respectively. Ethyl hexanoate
and neryl acetate were detected in all samples. Ethyl
hexanoate was present about the same quantity in
Guoqing 1 and Owari and the lowest quantities in
Miyagawa Wase fruit. Neryl acetate was the most predominant among the ester compounds in all samples,
and it occurred in higher proportions in Miyagawa Wase
fruit. Ethyl octanoate, linalyl acetate, citronellyl acetate,

1491

and geranyl acetate were the four common esters found

in both Guoqing 1 and Owari, and they were detected
in higher quantity in Guoqing 1.
Ketones and acids Ketones were believed to make a
positive contribution to the citrus flavor. The levels
of ketones in the three variety fruits were 0.18, 0.13,
and 0.18%, respectively. Carvone exhibited the highest concentration of ketones in all samples. Moreover,
acetic acid was detected in Owari.

DISCUSSION
Aroma compounds will make different contributions to
the fruit because of their thresholds and the concentrations in sample matrix. The contribution of chemical
compounds to food flavor is not judged by their content in sample. Only the compound possessing intense
aroma value could be the key aroma to the fruit (Zhang
et al. 2007). Elmaci and Altug (2005)detected 26 volatile
compounds in the three mandarin cultivars from Turkey using dynamic headspace, and the key aroma impact compounds were limonene, y-terpinene, p-cymene,
myrcene, a-pinene, P-pinene, and a-terpinolene in all
samples by sensory evaluation.

Terpenic compounds of characteristic aroma in

Satsuma mandarin varieties
Limonene accounted for the major proportion in citrus
aroma. Tgnder et al. (1998) pointed out that the limonene presenting typical citrus aroma was the most
important compound in orange juice. Because of its
low threshold and high content, limonene was considered to be the key aroma compound in the three selected Satsuma mandarin varieties.
Except for limonene, y-terpinene, P-myrcene, and
a-pinene are the abundant monoterpenic compounds
in Satsuma mandarin fruit. The odor thresholds of them
were low, and the three compounds have a citrusy,
balsamic, and piney note (Ahmed et al. 1978; Tgnder
et al. 1998; Plotto et al. 2004). Elmaci and Altug (2005)
also found them to contribute to the mandarin fruit.
Therefore, y-terpinene, P-myrcene, and a-pinene were
believed to be characteristic aroma compounds of selected samples.

02007, CAAS. All rights reserved. Publishedby Elsevier LM.

1492

Characteristic alcohol and aldehyde aroma

compounds

QIAO Yu et al.

studied further

CONCLUSION
Alcohols and aldehydes are the major aroma compounds
in citrus fruit. Among the alcohols and aldelhydes presented in this paper, linalool and octanal ranked the highest in terms of quantity. Linalool with fruity aroma
was the key aroma component in orange juice
(Nisperos-Carried0 and Shaw 1990). Linalool made a
positive contribution to orange flavor in combination as
per Ohta et al. (1982). Octanal is in general described
as the key aroma component in orange juice because of
typical citrus odor (Nisperos-Carried0 and Shaw 1990).
The study performed by Tgnder et al. (1998) showed
that the thresholds of linalool and octanal were only
lower than those of limonene. Both of them could make
a positive contribution to Satsuma mandarin flavor.

Fruit aromas of different varieties were analyzed by

headspace solid phase microextraction combined with
GC-MS. The results showed that there were 73, 71,
and 66 aroma components in the three varieties, the
compounds and amounts of hydrocarbons, alcohols,
aldehydes, and esters were dominant in Guoqing 1. The
contents of alcohols, esters, and ketones were lowest
in Miyagawa Wase and the quantities of hydrocarbons
and aldehydes were lowest in Owari. The key aroma
components were limonene, linalool, y-terpinene, pmyrcene, a-pinene, and octanal in the three fruits.
Guoqing 1 contained more amounts of key aroma compounds than Miyagawa Wase and Owari.

Other characteristic aroma compounds

Acknowledgements

Most of the esters exhibited fruity aroma, especially

some low boiled compounds, such as ethyl acetate and
ethyl butanoate. They have extremely low thresholds
but could not be detected in this study due to their high
volatility. Some ketones with lower quantities would
have effect on the aroma of Satsuma mandarin fruit.
The key aroma components were limonene, linalool,
y-terpinene, p-myrcene, a-pinene, and octanal in the
three Satsuma mandarin fruits. The difference of constitution in these compounds contributed to the variation of the overall aroma. By comparing the amounts
of these six key aroma compounds, we can see that
five compounds of them, except for a-pinene, were
presented in the highest quantities in Guoqing 1, followed by Miyagawa Wase and Owari. Therefore,
Guoqing 1 had relatively intense aroma, which is in accordance with the sensory evaluation. Moreover, the
total amounts and categories of aroma compounds in
Guoqing 1 were more than others. From these results,
it can be concluded that the aroma of Guoqing 1 was
the most prefered compared with Miyagawa Wase and
Owari.
Furthermore, the TSS/TA in Miyagawa Wase fruit
had higher quantities than other fruits, but the quantity
of aroma was lower than Guoqing 1 and Owari. The
correlation of taste and smell compounds will be still

The authors are grateful to the Wangchunhua Citrus

Valley Co., Ltd., China, for supplying citrus fruits. This
work was supported by the Project of Agriculture Structure Readjust of Ministry of Agriculture, China (04-09038) and the Major Key Technology R&D Program of
Hubei Province, China (2005AA201C68).

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(Edited by ZHANG Juan)

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